The influence of the electron donor tetrahydrofuran (THF) on the formation of the crystalline morphology of MgCl 2 was studied. MgCl 2 was synthesized from magnesium and 1-chlorobutane in the presence of THF with the THF/Mg molar ratio ranging from 0.063 to 2.0. With the highest amounts of THF crystalline particles were formed, as evidenced from scanning electron microscopy images. The X-ray structure analysis of these single crystals revealed the new organometallic Mg compound [Mg 3 Cl 5 (THF) 4 Bu] 2 (Bu = n-butyl), which has an open dicubanelike structure with four octahedrally and two tetrahedrally coordinated Mg atoms. The compound also contains two butyl groups directly bound to the Mg atoms at the opposite corners of the dicubane structure. With the lowest THF amounts, structurally disordered MgCl 2 /THF complexes were formed. The transition from single crystals toward particles with an amorphous morphology appeared to occur through an intermediate type of morphology with a three-dimensional network structure. The network structure is formed from a thin (30−100 nm) fiberlike MgCl 2 /THF material. Infrared and solid-state 13 C nuclear magnetic resonance spectroscopy measurements revealed different types of Mg sites present in the MgCl 2 /THF complexes.
For reliable function, bioelectrodes require a stable, low-impedance contact with the target tissue. In biosignal monitoring applications, in which low ion current densities are recorded, it is important to minimize electrode contact impedances. Recently, several flexible electrode concepts have been introduced for single-patient use. These electrodes conform well on the patient skin enabling an artifact-free, low-noise recording. In this study, polydimethylsiloxane (PDMS) elastomer was used as an electrode substrate material. One half of the substrates were surface-patterned with micropillars produced by using micro-working robot-made mold inserts and a replica molding technique. The substrates were subsequently coated with thin films of titanium (Ti), copper (Cu), silver (Ag) or silver–silver chloride (Ag/AgCl). Electrical impedance spectroscopy studies revealed that the micropillar structure caused statistically significant reductions in impedance modulus and phase for each coating candidate. The relative effect was strongest for pure Ag, for which the values of the real part (Z′) and the imaginary part (Z″) decreased to less than one tenth of the original (smooth) values. However, Ag/AgCl, as expected, proved to be a superior electrode material. Coating with chloride drastically reduced the interfacial impedance compared to pure Ag. Further significant reduction was achieved by the micropillars, since the phase angle declined from 10–13° (for smooth samples, f < 50 Hz) to a value as low as 5°. Equivalent circuit modeling was used to obtain a better understanding of phenomena occurring at various electrode–electrolyte interfaces. The knowledge obtained in this study will be exploited in the further development of flexible electrodes and miniaturized biointerfaces with improved electrochemical characteristics.
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